CN111234540A - A kind of low temperature resistant nanometer modified asphalt and preparation method thereof - Google Patents
A kind of low temperature resistant nanometer modified asphalt and preparation method thereofDownload PDFInfo
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Abstract
Translated fromChineseDescription
Translated fromChinese技术领域technical field
本发明涉及路面沥青材料技术领域，具体涉及一种耐低温纳米改性沥青及其制备方法。The invention relates to the technical field of pavement asphalt materials, in particular to a low temperature-resistant nano-modified asphalt and a preparation method thereof.
背景技术Background technique
高寒多年冻土地区沥青路面面临严重的低温收缩开裂和冻融循环疲劳损伤。该地区沥青路面面临严重的低温收缩、开裂和冻融循环疲劳损伤。由于它们在高空受到强烈的紫外线辐射，这将加速沥青老化并影响其使用寿命。而传统的改性沥青不能解决这一问题。Asphalt pavements in alpine permafrost areas face severe low-temperature shrinkage cracking and freeze-thaw cycle fatigue damage. Asphalt pavements in this region face severe low-temperature shrinkage, cracking, and freeze-thaw cycle fatigue damage. Since they are exposed to intense UV radiation at high altitudes, this will accelerate the aging of the asphalt and affect its service life. The traditional modified asphalt can not solve this problem.
胶粉常被用作沥青改性剂。它不仅能有效地改善路面性能，而且能充分利用废旧橡胶轮胎。近几十年来，为一种具有代表性的橡胶改性沥青技术，在世界范围内得到了广泛的研究和发展。胶粉改性沥青凭其在低温方面的强增韧效能被广泛应用。然而，其相容性不佳的问题始终存在，在生产、拌合等过程中易发生离析等现象，因而热稳定性无法兼顾，高温下易产生车辙等病害，无法保证路面长期耐久性。Rubber powder is often used as an asphalt modifier. It can not only effectively improve road performance, but also make full use of waste rubber tires. In recent decades, as a representative rubber-modified asphalt technology, it has been extensively researched and developed around the world. Rubber powder modified asphalt is widely used due to its strong and toughening performance at low temperature. However, the problem of poor compatibility always exists. Segregation and other phenomena are prone to occur in the process of production and mixing, so thermal stability cannot be taken into account, and diseases such as rutting are prone to occur at high temperatures, which cannot guarantee the long-term durability of the road surface.
液态丁苯橡胶(LSBR)作为丁二烯-苯乙烯共聚物，广泛应用于沥青改性在室温下能够兼具橡胶的高弹性和塑料的强塑性，已有研究表明，作为沥青改性剂的液体橡胶可提高基质沥青在低温下的应变松弛性能，且低温抗裂性较其大幅度改善。As a butadiene-styrene copolymer, liquid styrene-butadiene rubber (LSBR) is widely used in asphalt modification, which can combine the high elasticity of rubber and the strong plasticity of plastic at room temperature. Liquid rubber can improve the strain relaxation performance of matrix asphalt at low temperature, and its low temperature crack resistance is greatly improved.
但液体橡胶改性沥青在中高温环境下抗车辙能力欠佳，其粘性成分的大幅增加使得在高温环境中无法抵抗长期荷载，因此,橡胶沥青的高温性能和弹性严重下降，为实现了大幅改性沥青性能的目标，故研制一种具有耐低温橡胶改性沥青并能弥补其缺点的沥青材料，对于提高沥青路用性能和废旧轮胎利用具有重大意义。本发明拟将少量纳米二氧化硅作为LSBR改性的“催化剂”，以提高橡胶对沥青性能改性的上限。However, the rutting resistance of liquid rubber modified asphalt is not good in medium and high temperature environments, and the large increase in its viscous components makes it impossible to resist long-term loads in high temperature environments. Therefore, the high temperature performance and elasticity of rubber asphalt are seriously reduced. Therefore, it is of great significance to develop an asphalt material with low temperature resistance rubber modified asphalt that can make up for its shortcomings, which is of great significance for improving the performance of asphalt pavement and the utilization of waste tires. The present invention intends to use a small amount of nano-silica as a "catalyst" for LSBR modification, so as to improve the upper limit of the modification of asphalt performance by rubber.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种耐低温纳米改性沥青及其制备方法，解决了现有技术中存在的上述不足。The purpose of the present invention is to provide a low temperature-resistant nano-modified asphalt and a preparation method thereof, which solve the above-mentioned deficiencies in the prior art.
为了达到上述目的，本发明采用的技术方案是：In order to achieve the above object, the technical scheme adopted in the present invention is:
本发明提供的一种耐低温纳米改性沥青，包括以下原料：基质沥青100份、液体橡胶LSBR(0.5-6)份、纳米二氧化硅(1-7)份、稳定剂(1-3)份、岩沥青(15-20)份和石灰粉(2-4)份。The low-temperature-resistant nano-modified asphalt provided by the invention comprises the following raw materials: 100 parts of base asphalt, (0.5-6) parts of liquid rubber LSBR, (1-7) parts of nano-silica, and (1-3) parts of stabilizer parts, rock asphalt (15-20) parts and lime powder (2-4) parts.
优选地，所述液体橡胶LSBR为2万分子量LSBR时，2万分子量LSBR为(1-6)份。Preferably, when the liquid rubber LSBR is 20,000 molecular weight LSBR, the 20,000 molecular weight LSBR is (1-6) parts.
优选地，所述液体橡胶LSBR为5万分子量LSBR时，5万分子量LSBR为(0.5-4)份。Preferably, when the liquid rubber LSBR is 50,000 molecular weight LSBR, the 50,000 molecular weight LSBR is (0.5-4) parts.
优选地，所述基质沥青为70#基质沥青或SK90#基质沥青。Preferably, the base asphalt is 70# base asphalt or SK90# base asphalt.
优选地，所述纳米二氧化硅为JH-silica。Preferably, the nano-silica is JH-silica.
优选地，所述稳定剂为混合物、硫磺和含硫有机化合物中的一种或几种；所述混合物由亚油酸钠25份、硅藻土25份和硫磺粉末50份组成。Preferably, the stabilizer is one or more of a mixture, sulfur and a sulfur-containing organic compound; the mixture is composed of 25 parts of sodium linoleate, 25 parts of diatomaceous earth and 50 parts of sulfur powder.
一种耐低温纳米改性沥青的制备方法，基于所述的一种耐低温纳米改性沥青，包括以下步骤：A preparation method of low temperature-resistant nano-modified asphalt, based on the low-temperature-resistant nano-modified asphalt, comprising the following steps:
步骤1，将称取的基质沥青加热至熔融状态；Step 1, heating the weighed base asphalt to a molten state;
步骤2，在恒温下，向熔融状态的基质沥青中加入液体橡胶LSBR并进行搅拌直至呈固融态；室温静置、保持干燥，得到橡胶改性沥青；
步骤3，将步骤3中得到橡胶改性沥青加热至熔融状态后，依次加入纳米二氧化硅与岩沥青，采用循环式进行剪切研磨，得到混溶物；Step 3, after heating the rubber-modified asphalt obtained in step 3 to a molten state, adding nano-silica and rock asphalt in turn, and shearing and grinding in a cyclic manner to obtain a miscible;
步骤4，将稳定剂、石灰粉末加入到步骤4中得到的混溶物中，进行剪切搅拌，得到纳米改性沥青。In step 4, the stabilizer and lime powder are added to the mixture obtained in step 4, and shearing and stirring are performed to obtain nano-modified asphalt.
优选地，步骤4中，采用循环式进行剪切研磨的具体工艺是：在130℃-180℃温度下，每隔5-10min，以1500～8000r/min的转速进行高速剪切搅拌5-20min；以此循环2～4次。Preferably, in step 4, the specific process for shearing and grinding in a cyclic manner is: at a temperature of 130°C-180°C, at a temperature of 130°C-180°C, high-speed shearing and stirring are performed at a rotational speed of 1500-8000 r/min for 5-20 minutes every 5-10 minutes. ; This
优选地，步骤5中，剪切搅拌的工艺条件是：在140℃-165℃温度下，以1500～8000r/min的转速剪切搅拌。Preferably, in step 5, the process conditions for shearing and stirring are: shearing and stirring at a rotational speed of 1500-8000 r/min at a temperature of 140°C-165°C.
与现有技术相比，本发明的有益效果是：Compared with the prior art, the beneficial effects of the present invention are:
本发明提供的一种耐低温纳米改性沥青及其制备方法，通过液体橡胶LSBR和疏水性纳米二氧化硅粒子的混合下，可以明显改善基质沥青的低温断裂韧性；从物理性能角度来看，橡胶颗粒的空化和基体剪切变形引起的空穴生长是一种重要的增韧机制。橡胶相的泊松比大于沥青胶体，橡胶颗粒的横向收缩和热膨胀系数也大于沥青横向收缩，因而当温度冷却至室温后橡胶相收缩大于基体相，两相之间的界面区域中的自由体积的增加，引起橡胶颗粒在微观尺度的空化，便是液体橡胶沥青增韧的关键作用；而纳米粒子的增韧抗裂原理从微观尺度可以用塑化空隙生长的理论来解释，这种非平面化的形态在沥青结合料的低温松弛性能改善方面作用显著。进一步的，认为纳米粒子从液体橡胶基体中脱粘过程中的能耗对纳米改性沥青的低温柔性起着重要的影响；混合填料在橡胶基体均匀分散,加强了填料与基体的界面作用，建立良好的三维空间网络结构，使复合材料在高温下具有足够模量，其回弹性能得到改善；The low temperature-resistant nano-modified asphalt and its preparation method provided by the invention can obviously improve the low-temperature fracture toughness of the base asphalt by mixing the liquid rubber LSBR and the hydrophobic nano-silica particles; Cavitation of rubber particles and growth of voids caused by shear deformation of the matrix are an important toughening mechanism. The Poisson's ratio of the rubber phase is greater than that of the asphalt colloid, and the lateral shrinkage and thermal expansion coefficient of the rubber particles are also greater than the lateral shrinkage of the asphalt. Therefore, when the temperature is cooled to room temperature, the rubber phase shrinks more than the matrix phase, and the free volume in the interface area between the two phases is smaller than that of the matrix phase. Increase, causing the cavitation of rubber particles at the micro-scale, is the key role in the toughening of liquid rubber asphalt; and the toughening and cracking principle of nanoparticles can be explained from the micro-scale by the theory of plasticized void growth. The modified morphology plays a significant role in the improvement of the low-temperature relaxation properties of the asphalt binder. Further, it is believed that the energy consumption during the debonding process of nanoparticles from the liquid rubber matrix plays an important role in the low temperature flexibility of the nano-modified asphalt; the mixed fillers are uniformly dispersed in the rubber matrix, which strengthens the interface between the filler and the matrix. The good three-dimensional spatial network structure makes the composite material have sufficient modulus at high temperature, and its resilience performance is improved;
从化学反应的角度来看，在高速剪切的状态下，兼具高比表能的纳米粒子能够最大效能的与基体吸附黏结，因而该纳米改性沥青的高温抗剪能力大幅增强。但未经表面处理的纳米二氧化硅的强亲水性导致了其难以在有机相中润湿和分散，限制了其纳米效应的充分发挥。硅烷改性的材料可以在表面形成有机偶联剂，骨料变为亲油性，为加强沥青与骨料之间的界面固结提供了基础。因此，复合改性沥青的机械强度和韧性均比基质沥青好，并且具有良好的高温性能，抗衰老，抗疲劳和其他特性。表面改性后，纳米二氧化硅的接触角达到70°至150°。From the point of view of chemical reaction, in the state of high-speed shearing, the nanoparticles with high specific surface energy can adsorb and bond with the matrix with maximum efficiency, so the high-temperature shearing resistance of the nano-modified asphalt is greatly enhanced. However, the strong hydrophilicity of nano-silica without surface treatment makes it difficult to wet and disperse in the organic phase, which limits the full play of its nano-effect. The silane-modified material can form an organic coupling agent on the surface, and the aggregate becomes lipophilic, which provides a basis for strengthening the interfacial consolidation between asphalt and aggregate. Therefore, composite modified asphalt has better mechanical strength and toughness than matrix asphalt, and has good high temperature performance, anti-aging, anti-fatigue and other properties. After surface modification, the contact angle of nano-silica reaches 70° to 150°.
附图说明Description of drawings
图1是实施例1至实施例5中改性沥青的蠕变速率；Fig. 1 is the creep rate of modified asphalt in Example 1 to Example 5;
图2是实施例6、实施例7与对比例1、对比例2、对比例3中改性沥青的蠕变速率；Fig. 2 is the creep rate of modified asphalt in Example 6, Example 7 and Comparative Example 1, Comparative Example 2, and Comparative Example 3;
图3是实施例1至实施例5中改性沥青的劲度模量；Fig. 3 is the stiffness modulus of modified asphalt in Examples 1 to 5;
图4是实施例6、实施例7与对比例1、对比例2、对比例3中改性沥青的劲度模量。4 is the stiffness modulus of modified asphalt in Example 6, Example 7 and Comparative Example 1, Comparative Example 2, and Comparative Example 3.
具体实施方式Detailed ways
下面结合附图，对本发明进一步详细说明。The present invention will be described in further detail below with reference to the accompanying drawings.
本发明提供的一种耐低温纳米改性沥青，按照重量份计，包括以下原料：基质沥青100份、液体橡胶LSBR(0.5-6)份、纳米二氧化硅(1-7)份、稳定剂(1-3)份、岩沥青(15-20)份和石灰粉(2-4)份。The low-temperature-resistant nano-modified asphalt provided by the present invention comprises, in parts by weight, the following raw materials: 100 parts of base asphalt, (0.5-6) parts of liquid rubber LSBR, (1-7) parts of nano-silica, and stabilizer (1-3) parts, rock asphalt (15-20) parts and lime powder (2-4) parts.
当所述液体橡胶LSBR为2万分子量LSBR时，2万分子量LSBR为(1-6)份。When the liquid rubber LSBR is 20,000 molecular weight LSBR, the 20,000 molecular weight LSBR is (1-6) parts.
当所述液体橡胶LSBR为5万分子量LSBR时，5万分子量LSBR为(0.5-4)份。When the liquid rubber LSBR is 50,000 molecular weight LSBR, the 50,000 molecular weight LSBR is (0.5-4) parts.
所述LSBR采用负离子聚合法制备，为调控苯乙烯在聚合物长链上的分布，加入了四氢呋喃这类无规化试剂，得到一种丁二烯和苯乙烯的低相对分子质量共聚物，可替代低分子油类起增塑剂或软化剂的功效。The LSBR is prepared by anion polymerization. In order to regulate the distribution of styrene on the long polymer chain, randomizing agents such as tetrahydrofuran are added to obtain a low relative molecular weight copolymer of butadiene and styrene, which can be Substitute low-molecular-weight oils to act as plasticizers or softeners.
所述基质沥青采用中海70#基质沥青或韩国SK90#基质沥青。The base asphalt adopts Zhonghai 70# base asphalt or Korea SK90# base asphalt.
所述纳米二氧化硅为硅烷偶联剂处理后的JH-silica，JH-N318对纳米二氧化硅进行表面化学改性，其化学分子式CH3(CH2)7Si(OCH3)3，可与纳米二氧化硅表面-OH反应，在其表面引入有机链，从而改变纳米粒子的性能。其有机部分碳链比其他硅烷偶联剂更长，空间位阻更大，因而可以进一步阻止纳米粒子之间团聚。The nano-silica is JH-silica treated with a silane coupling agent, and JH-N318 has chemically modified the surface of the nano-silica, and its chemical formula is CH3 (CH2 )7 Si(OCH3 )3 , which can be Reacts with -OH on the surface of nano-silica to introduce organic chains on its surface, thereby changing the properties of nanoparticles. Its organic carbon chain is longer than other silane coupling agents, and the steric hindrance is larger, which can further prevent the agglomeration between nanoparticles.
所述石灰粉末可以调节沥青的固化时间与固化状态。The lime powder can adjust the curing time and curing state of the asphalt.
所述岩沥青作为一种天然沥青，其掺入使得改性沥青在高温稳定性方面能够得到显著提高和改善，低温性能较单纯的基质沥青也得到了相当程度的改善。The rock asphalt is a kind of natural asphalt, and the incorporation of the rock asphalt can significantly improve and improve the high temperature stability of the modified asphalt, and the low temperature performance of the matrix asphalt can also be improved to a considerable extent.
所述稳定剂为混合物、硫磺和含硫有机化合物中的一种或几种；所述混合物由亚油酸钠25份、硅藻土25份和硫磺粉末50份组成。The stabilizer is one or more of mixture, sulfur and sulfur-containing organic compounds; the mixture is composed of 25 parts of sodium linoleate, 25 parts of diatomaceous earth and 50 parts of sulfur powder.
本发明提供的一种抗低温的纳米改性沥青的制备方法，包括以下步骤：A preparation method of a low temperature resistant nano-modified asphalt provided by the present invention comprises the following steps:
步骤1、按照质量份数称取基质沥青、纳米二氧化硅、岩沥青、稳定剂、石灰粉和液体橡胶LSBR；其中，所述稳定剂为混合物、硫磺和含硫有机化合物中的一种或几种；所述混合物由亚油酸钠25份、硅藻土25份和硫磺粉末50份组成；Step 1, take by weighing matrix asphalt, nano-silicon dioxide, rock asphalt, stabilizer, lime powder and liquid rubber LSBR according to parts by mass; wherein, the stabilizer is a kind of mixture, sulfur and sulfur-containing organic compound or several; the mixture is composed of 25 parts of sodium linoleate, 25 parts of diatomaceous earth and 50 parts of sulfur powder;
步骤2、将基质沥青加热至熔融状态并保温；
步骤3、将恒温油浴锅设在60℃上，将基质沥青置于其中，待温度恒定后向其中掺入液体橡胶LSBR，人工搅拌，此时改性沥青应呈粘滞阻力较强的固融态，保持匀速人工搅拌20-30min，拌速为190-200r/min，室温静置2h，保持干燥，得到橡胶改性沥青；Step 3. Set the constant temperature oil bath pot at 60°C, place the base asphalt in it, mix liquid rubber LSBR into it after the temperature is constant, and stir manually. At this time, the modified asphalt should be solid with strong viscous resistance. In the melted state, keep stirring at a constant speed for 20-30 minutes manually, at a mixing speed of 190-200 r/min, let it stand for 2 hours at room temperature, and keep it dry to obtain rubber-modified asphalt;
步骤4、将步骤3中得到橡胶改性沥青加热至熔融状态后，依次加入纳米二氧化硅与岩沥青，采用循环式进行剪切研磨，得到混溶物；Step 4. After heating the rubber-modified asphalt obtained in step 3 to a molten state, add nano-silica and rock asphalt in turn, and perform shear grinding in a cyclic manner to obtain a miscible;
步骤5、将稳定剂、石灰粉末加入到步骤4中得到的混溶物中，进行剪切搅拌，得到纳米改性沥青。Step 5. Add stabilizer and lime powder to the miscible obtained in step 4, and perform shearing and stirring to obtain nano-modified asphalt.
其中，步骤2中，基质沥青的加热温度控制在100-180℃之间，优选135℃-155℃。Wherein, in
步骤4中，采用循环式进行剪切研磨的具体工艺是：在130℃-180℃温度下，优选145℃-165℃；每隔5-10min，进行高速剪切搅拌5-20min，按此方法循环2～4次，并控制剪切时间的上限为105min，因为搅拌时间过长耗能过高；该过程剪切机将转速设定为1500～8000r/min，优选为3500-6000r/min；In step 4, the specific process of shearing and grinding in a cyclic manner is: at a temperature of 130°C-180°C, preferably 145°C-165°C; every 5-10min, carry out high-speed shearing and stirring for 5-20min, according to this method. Circulate 2 to 4 times, and control the upper limit of the shearing time to 105min, because the stirring time is too long and the energy consumption is too high; in this process, the speed of the shearing machine is set to 1500-8000r/min, preferably 3500-6000r/min;
步骤5中，剪切搅拌的工艺条件是：温度控制在140℃-165℃之间，该过程剪切机将转速设定为1500～8000r/min，优选剪切速率为3500-6000r/min；搅拌时间为25～30min。In step 5, the process conditions of shearing and stirring are: the temperature is controlled between 140°C and 165°C, and the shearing machine in this process is set to rotate at a speed of 1500-8000r/min, preferably a shearing rate of 3500-6000r/min; The stirring time is 25-30 min.
本发明有益效果：Beneficial effects of the present invention:
通过液体橡胶(LSBR)和疏水性纳米二氧化硅粒子的混合下，可以明显改善基质沥青的低温断裂韧性。By mixing liquid rubber (LSBR) and hydrophobic nano-silica particles, the low temperature fracture toughness of the base asphalt can be significantly improved.
从物理性能角度来看，橡胶颗粒的空化和基体剪切变形引起的空穴生长是一种重要的增韧机制。橡胶相的泊松比大于沥青胶体，橡胶颗粒的横向收缩和热膨胀系数也大于沥青横向收缩，因而当温度冷却至室温后橡胶相收缩大于基体相，两相之间的界面区域中的自由体积的增加，引起橡胶颗粒在微观尺度的空化，便是液体橡胶沥青增韧的关键作用；而纳米粒子的增韧抗裂原理从微观尺度可以用塑化空隙生长的理论来解释，这种非平面化的形态在沥青结合料的低温松弛性能改善方面作用显著。进一步的，认为纳米粒子从液体橡胶基体中脱粘过程中的能耗对纳米改性沥青的低温柔性起着重要的影响。混合填料在橡胶基体均匀分散,加强了填料与基体的界面作用,建立良好的三维空间网络结构,使复合材料在高温下具有足够模量，其回弹性能得到改善。From the perspective of physical properties, the cavitation of rubber particles and the growth of voids caused by shear deformation of the matrix are an important toughening mechanism. The Poisson's ratio of the rubber phase is greater than that of the asphalt colloid, and the lateral shrinkage and thermal expansion coefficient of the rubber particles are also greater than the lateral shrinkage of the asphalt. Therefore, when the temperature is cooled to room temperature, the rubber phase shrinks more than the matrix phase, and the free volume in the interface area between the two phases is smaller than that of the matrix phase. Increase, causing the cavitation of rubber particles at the micro-scale, is the key role in the toughening of liquid rubber asphalt; and the toughening and cracking principle of nanoparticles can be explained from the micro-scale by the theory of plasticized void growth. The modified morphology plays a significant role in the improvement of the low-temperature relaxation properties of the asphalt binder. Furthermore, it is believed that the energy consumption during the debonding of nanoparticles from the liquid rubber matrix plays an important role in the low temperature flexibility of the nano-modified asphalt. The mixed filler is uniformly dispersed in the rubber matrix, which strengthens the interface between the filler and the matrix, and establishes a good three-dimensional spatial network structure, so that the composite material has sufficient modulus at high temperature, and its resilience performance is improved.
从化学反应的角度来看，在高速剪切的状态下，兼具高比表能的纳米粒子能够最大效能的与基体吸附黏结，因而该纳米改性沥青的高温抗剪能力大幅增强。但纳米二氧化硅的强亲水性导致了其难以在有机相中润湿和分散，限制了其纳米效应的充分发挥。硅烷改性的材料可以在表面形成有机偶联剂，骨料由疏水性变为亲油性，为加强沥青与骨料之间的界面固结提供了基础。因此，复合改性沥青的机械强度和韧性均比基质沥青好，并且具有良好的高温性能，抗衰老，抗疲劳和其他特性。表面改性后，纳米二氧化硅的接触角达到70°至150°。From the point of view of chemical reaction, in the state of high-speed shearing, the nanoparticles with high specific surface energy can adsorb and bond with the matrix with maximum efficiency, so the high-temperature shearing resistance of the nano-modified asphalt is greatly enhanced. However, the strong hydrophilicity of nano-silica makes it difficult to wet and disperse in the organic phase, which limits the full play of its nano-effect. The silane-modified material can form an organic coupling agent on the surface, and the aggregate changes from hydrophobicity to lipophilicity, which provides a basis for strengthening the interface consolidation between asphalt and aggregate. Therefore, composite modified asphalt has better mechanical strength and toughness than matrix asphalt, and has good high temperature performance, anti-aging, anti-fatigue and other properties. After surface modification, the contact angle of nano-silica reaches 70° to 150°.
实施例1Example 1
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，2万分子量LSBR2份，石灰粉末1份，稳定剂2.5份，岩沥青17.5份，JH-silica3份；The raw materials of nano-modified asphalt in this embodiment are calculated as follows in terms of mass fraction: 100 parts of No. 90 road petroleum asphalt, 2 parts of 20,000 molecular weight LSBR, 1 part of lime powder, 2.5 parts of stabilizer, 17.5 parts of rock asphalt, and 3 parts of JH-silica;
将500份基质沥青加热到165℃，加入2份的2w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，此时改性沥青应呈粘滞阻力较强的固融态，然后室温静置2h。然后将橡胶改性沥青加热至145℃上下，此时沥青应呈熔融流动状态，将17.5份岩沥青与3份JH-silica加入沥青中得到共混物，进行剪切研磨，搅拌均匀该混合物中,此时降温至155℃，每隔5min高速剪切搅拌10min，此周期循环四次，最高剪切速率5000r/min，剪切时间为60min；之后再加入2.5份稳定剂和1份石灰粉末，进行剪切搅拌，最高剪切速率6900r/min,搅拌30min后完成样品的制备。
实施例2Example 2
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，2万分子量LSBR3份，石灰粉末0.5份，稳定剂2份，岩沥青15份，JH-silica4份。The raw materials of nano-modified asphalt in this example are calculated by mass fraction: 100 parts of No. 90 road petroleum asphalt, 3 parts of 20,000 molecular weight LSBR, 0.5 parts of lime powder, 2 parts of stabilizer, 15 parts of rock asphalt, and 4 parts of JH-silica.
将500份基质沥青加热到160℃，加入3份的2w-LSBR，油浴箱恒温70℃进行人工搅拌，搅速为195r/min，保持匀速搅拌，然后室温静置2h。将橡胶改性沥青加热至137℃上下，将15份岩沥青与4份JH-silica加入其中得到共混物，进行剪切研磨，搅拌均匀该混合物中,此时升温至165℃，每隔10min高速剪切搅拌10min，此周期循环四次，最高剪切速率5500r/min，剪切时间为80min；之后再加入2份稳定剂和0.5份石灰粉末，进行剪切搅拌，最高剪切速率6000r/min,搅拌30min后完成样品的制备。
实施例3Example 3
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，5万分子量LSBR2份，石灰粉末3份，稳定剂2份，岩沥青18份，JH-silica4份。The raw materials of nano-modified asphalt in this example are calculated as: 100 parts of No. 90 road petroleum asphalt, 2 parts of 50,000 molecular weight LSBR, 3 parts of lime powder, 2 parts of stabilizer, 18 parts of rock asphalt, and 4 parts of JH-silica.
将500份基质沥青加热到160℃，加入2份的5w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，室温静置2h。将橡胶改性沥青加热至130℃，将18份岩沥青与4份JH-silica加入其中得到共混物，进行剪切研磨，加入剪切研磨，搅拌均匀该混合物中,此时升温至163℃，每隔10min高速剪切搅拌15min，此周期循环2次，最高剪切速率5400r/min，剪切时间为50min；之后再加入2份稳定剂和3份石灰粉末，进行剪切搅拌，最高剪切速率7000r/min,搅拌30min后完成样品的制备。500 parts of base asphalt were heated to 160°C, 2 parts of 5w-LSBR were added, the oil bath was kept at a constant temperature of 60°C for manual stirring, the stirring speed was 200r/min, the stirring was maintained at a constant speed, and the room temperature was allowed to stand for 2h. The rubber-modified asphalt was heated to 130°C, 18 parts of rock asphalt and 4 parts of JH-silica were added to obtain a blend, which was sheared and ground, added to the sheared and ground, and stirred evenly into the mixture, and the temperature was raised to 163°C at this time. , high-speed shearing and stirring for 15min every 10min, this cycle is cycled twice, the maximum shear rate is 5400r/min, and the shearing time is 50min; then 2 parts of stabilizer and 3 parts of lime powder are added for shearing and stirring, and the maximum shearing time is 50 minutes. The shear rate was 7000 r/min, and the sample preparation was completed after stirring for 30 min.
实施例4Example 4
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，2万分子量LSBR1份，石灰粉末1份，稳定剂3份，岩沥青15份和JH-silica6份。The raw materials of nano-modified asphalt in this example are calculated as: 100 parts of No. 90 road petroleum asphalt, 1 part of 20,000 molecular weight LSBR, 1 part of lime powder, 3 parts of stabilizer, 15 parts of rock asphalt and 6 parts of JH-silica.
将500份基质沥青加热到160℃，加入1份的2w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，室温静置2h。将橡胶改性沥青加热至145℃，将15份岩沥青和6份JH-silica加入剪切研磨，搅拌均匀该混合物中,此时升温至163℃，每隔10min高速剪切搅拌20min，此周期循环2次，最高剪切速率4000r/min，剪切时间为60min；之后再加入3份稳定剂和1份石灰粉末，进行剪切搅拌，最高剪切速率8000r/min,搅拌30min后完成样品的制备。500 parts of base asphalt were heated to 160°C, 1 part of 2w-LSBR was added, and the oil bath was kept at a constant temperature of 60°C for manual stirring. Heat the rubber-modified asphalt to 145°C, add 15 parts of rock asphalt and 6 parts of JH-silica to the mixture for shearing and grinding, and stir evenly into the mixture. At this time, the temperature is raised to 163°C, and high-speed shearing and stirring for 20 minutes are carried out every 10 minutes. Circulate 2 times, the maximum shear rate is 4000r/min, and the shearing time is 60min; after that, 3 parts of stabilizer and 1 part of lime powder are added to carry out shear stirring, the maximum shear rate is 8000r/min, and the sample is stirred for 30min. preparation.
实施例5Example 5
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，5万分子量LSBR1份，石灰粉末3份，稳定剂3份，岩沥青15份和JH-silica4份。The raw materials of nano-modified asphalt in this example are calculated by mass fraction: 100 parts of No. 90 road petroleum asphalt, 1 part of LSBR with a molecular weight of 50,000, 3 parts of lime powder, 3 parts of stabilizer, 15 parts of rock asphalt and 4 parts of JH-silica.
将500份基质沥青加热到155℃，加入1份的5w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，室温静置2h。将橡胶改性沥青加热至145℃，将15份岩沥青和4份JH-silica加入剪切研磨，搅拌均匀该混合物中,此时升温至165℃，每隔10min高速剪切搅拌20min，此周期循环2次，最高剪切速率4000r/min，剪切时间为60min；之后再加入3份稳定剂和3份石灰粉末，进行剪切搅拌，最高剪切速率6000r/min,搅拌25min后完成样品的制备。500 parts of base asphalt was heated to 155°C, 1 part of 5w-LSBR was added, and the oil bath was kept at a constant temperature of 60°C for manual stirring at a stirring speed of 200 r/min. Heat the rubber-modified asphalt to 145°C, add 15 parts of rock asphalt and 4 parts of JH-silica to the mixture for shearing and grinding, and stir evenly into the mixture. At this time, the temperature is raised to 165°C, and high-speed shearing and stirring for 20 minutes are carried out every 10 minutes. Circulate 2 times, the maximum shear rate is 4000r/min, and the shearing time is 60min; then 3 parts of stabilizer and 3 parts of lime powder are added for shearing and stirring, the maximum shear rate is 6000r/min, and the sample is stirred for 25min. preparation.
实施例6Example 6
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，5万分子量LSBR1.5份，石灰粉末1份，稳定剂2.5份，岩沥青17.5份和JH-silica2.5份。The raw materials of nano-modified asphalt in this example are calculated as: 100 parts of No. 90 road petroleum asphalt, 1.5 parts of LSBR with a molecular weight of 50,000, 1 part of lime powder, 2.5 parts of stabilizer, 17.5 parts of rock asphalt and 2.5 parts of JH-silica share.
将500份基质沥青加热到165℃，加入1.5份的5w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为195r/min，保持匀速搅拌，然后室温静置2h。然后将橡胶改性沥青加热至155℃上下，此时沥青应呈熔融流动状态，将17.5份岩沥青与2.5份JH-silica加入剪切研磨，搅拌均匀该混合物中,此时降温至150℃，每隔10min高速剪切搅拌10min，此周期循环4次，最高剪切速率6000r/min，剪切时间为60min；之后再加入2.5份和稳定剂1份石灰粉末，进行剪切搅拌，最高剪切速率7000r/min,搅拌30min后完成样品的制备。500 parts of base asphalt was heated to 165 ℃, 1.5 parts of 5w-LSBR was added, and the oil bath was kept at a constant temperature of 60 ℃ for manual stirring, and the stirring speed was 195 r/min. Then heat the rubber-modified asphalt to around 155°C. At this time, the asphalt should be in a molten and flowing state. Add 17.5 parts of rock asphalt and 2.5 parts of JH-silica to the mixture for shearing and grinding, and stir evenly into the mixture. High-speed shearing and stirring for 10min every 10min, this cycle is cycled 4 times, the maximum shear rate is 6000r/min, and the shearing time is 60min; after that, 2.5 parts of lime powder and 1 part of stabilizer are added for shearing and stirring. The speed of 7000r/min, the preparation of the sample was completed after stirring for 30min.
实施例7Example 7
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，5万分子量LSBR1.5份，石灰粉末3份，稳定剂4份，岩沥青17份和JH-silica1份。The raw materials of nano-modified asphalt in this example are calculated as follows: 100 parts of No. 90 road petroleum asphalt, 1.5 parts of LSBR with a molecular weight of 50,000, 3 parts of lime powder, 4 parts of stabilizer, 17 parts of rock asphalt and 1 part of JH-silica.
将500份基质沥青加热到163℃，加入1.5份的5w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，室温静置2h。将橡胶改性沥青加热至155℃，此时将17份岩沥青与1份JH-silica共同加入其中进行剪切研磨，搅拌均匀该混合物中,此时保持恒温至155℃，每隔5min高速剪切搅拌10min，此周期循环四次，最高剪切速率6500r/min，剪切时间为60min；之后再加入4份稳定剂与3份石灰粉末，进行剪切搅拌，最高剪切速率7000r/min,搅拌30min后完成样品的制备。500 parts of base asphalt was heated to 163 ℃, 1.5 parts of 5w-LSBR was added, the oil bath was kept at a constant temperature of 60 ℃ for manual stirring, the stirring speed was 200 r/min, the stirring was kept at a constant speed, and the room temperature was allowed to stand for 2 hours. The rubber-modified asphalt was heated to 155°C, 17 parts of rock asphalt and 1 part of JH-silica were added together for shearing and grinding, and the mixture was stirred evenly. Cut and stir for 10min, this cycle is cycled four times, the maximum shear rate is 6500r/min, and the shear time is 60min; then 4 parts of stabilizer and 3 parts of lime powder are added for shearing and stirring, the maximum shear rate is 7000r/min, The preparation of the sample was completed after stirring for 30 min.
对比例1Comparative Example 1
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份；2万分子量LSBR2份；石灰粉1份；稳定剂2.5份；岩沥青17.5份；The raw materials of nano-modified asphalt in this embodiment are calculated as follows: 100 parts of No. 90 road petroleum asphalt; 2 parts of 20,000 molecular weight LSBR; 1 part of lime powder; 2.5 parts of stabilizer; 17.5 parts of rock asphalt;
将100份的基质沥青加热到165℃，加入2份的2w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，此时改性沥青应呈粘滞阻力较强的固融态，然后室温静置2h。
然后将橡胶改性沥青加热至145℃上下，此时沥青应呈熔融流动状态，将17.5份的岩沥青加入剪切研磨，搅拌均匀该混合物中,此时降温至155℃，每隔5min高速剪切搅拌10min，此周期循环四次，最高剪切速率5000r/min，剪切时间为60min；之后再加入2.5份稳定剂、1份石灰粉末，进行剪切搅拌，最高剪切速率6900r/min,搅拌30min后完成样品的制备。Then heat the rubber-modified asphalt to about 145°C. At this time, the asphalt should be in a molten and flowing state. Add 17.5 parts of rock asphalt into the mixture for shear grinding and stir it evenly. At this time, the temperature is lowered to 155°C, and high-speed shearing is performed every 5 minutes. Cut and stir for 10min, this cycle is cycled four times, the maximum shear rate is 5000r/min, and the shear time is 60min; after that, 2.5 parts of stabilizer and 1 part of lime powder are added for shearing and stirring, the maximum shear rate is 6900r/min, The preparation of the sample was completed after stirring for 30 min.
对比例2Comparative Example 2
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，2万分子量LSBR3份，石灰粉末0.5份，稳定剂2份，岩沥青15份。The raw materials of nano-modified asphalt in this example are calculated as: 100 parts of No. 90 road petroleum asphalt, 3 parts of 20,000 molecular weight LSBR, 0.5 parts of lime powder, 2 parts of stabilizer, and 15 parts of rock asphalt.
将500份基质沥青加热到160℃，加入3份的2w-LSBR，油浴箱恒温70℃进行人工搅拌，搅速为195r/min，保持匀速搅拌，然后室温静置2h。将橡胶改性沥青加热至137℃上下，将15份岩沥青加入剪切研磨，搅拌均匀该混合物中,此时升温至165℃，每隔10min高速剪切搅拌10min，此周期循环四次，最高剪切速率5500r/min，剪切时间为80min，之后加入2份稳定剂和0.5份石灰粉末，进行剪切搅拌，最高剪切速率6000r/min,搅拌30min后完成样品的制备。
对比例3Comparative Example 3
本实施例纳米改性沥青原料按照质量分数计为：90号道路石油沥青100份，5万分子量LSBR2份，石灰粉末3份，稳定剂2份，岩沥青18份。The raw materials of nano-modified asphalt in this example are calculated by mass fraction: 100 parts of No. 90 road petroleum asphalt, 2 parts of LSBR with a molecular weight of 50,000, 3 parts of lime powder, 2 parts of stabilizer, and 18 parts of rock asphalt.
将500份基质沥青加热到160℃，加入2份的5w-LSBR，油浴箱恒温60℃进行人工搅拌，搅速为200r/min，保持匀速搅拌，室温静置2h。将橡胶改性沥青加热至130℃，将18份岩沥青加入剪切研磨，搅拌均匀该混合物中,此时升温至163℃，每隔10min高速剪切搅拌15min，此周期循环2次，最高剪切速率5400r/min，剪切时间为50min，之后再加入2份稳定剂和3份石灰粉末，进行剪切搅拌，最高剪切速率7000r/min,搅拌30min后完成样品的制备。500 parts of base asphalt were heated to 160°C, 2 parts of 5w-LSBR were added, the oil bath was kept at a constant temperature of 60°C for manual stirring, the stirring speed was 200r/min, the stirring was maintained at a constant speed, and the room temperature was allowed to stand for 2h. Heat the rubber-modified asphalt to 130°C, add 18 parts of rock asphalt into the mixture for shear grinding, and stir evenly into the mixture. At this time, the temperature is raised to 163°C, and the high-speed shearing and stirring are performed for 15 minutes every 10 minutes. The shear rate is 5400r/min, the shearing time is 50min, and then 2 parts of stabilizer and 3 parts of lime powder are added for shearing and stirring, the maximum shear rate is 7000r/min, and the preparation of the sample is completed after stirring for 30min.
下面对实施例1-7，对比例1-3样品进行性能测试。The performance test of the samples of Examples 1-7 and Comparative Examples 1-3 is carried out below.
测试实验结果包括实施例样品的针入度、软化点、延度(低温延度，取5℃)及-12℃，-18℃、-24℃下用弯曲梁流变试验仪(BBR)特定的评价该抗低温纳米改性沥青的耐低温效果，具体参照JTG E20-2011《公路工程沥青及沥青混合料试验规程》。The test results include the penetration, softening point, ductility (low temperature ductility, take 5°C) of the samples of the examples, and are specified by a bending beam rheometer (BBR) at -12°C, -18°C, and -24°C. To evaluate the low temperature resistance effect of the low temperature resistant nano-modified asphalt, refer to JTG E20-2011 "Asphalt and Asphalt Mixture Test Regulations for Highway Engineering".
表1三大指标实验结果Table 1 Experimental results of three major indicators
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